L-Proline, ethyl ester → Pyrrolidinium, 1-(1,3-dithiol-2-ylidene)-2-(ethoxycarbonyl)-, perchlorate

HRID 648919

反応式

HRID 648919 の反応式
[CH2:1]([O:3][C:4](=[O:10])[C@@H:5]1[CH2:9][CH2:8][CH2:7][NH:6]1)[CH3:2].[Cl:11]([O-:15])(=[O:14])(=[O:13])=[O:12].CS[C:18]1[S:22][CH:21]=[CH:20][S+:19]=1>O1CCCC1>[Cl:11]([O-:15])(=[O:14])(=[O:13])=[O:12].[S:19]1[CH:20]=[CH:21][S:22][C:18]1=[N+:6]1[CH2:7][CH2:8][CH2:9][CH:5]1[C:4]([O:3][CH2:1][CH3:2])=[O:10]

参加物

4

反応物 2

HCID 79888L-Proline, ethyl esterHCID 230390092-Methylthio-1,3-dithiolium perchlorate

生成物 1

HCID 3064796Pyrrolidinium, 1-(1,3-dithiol-2-ylidene)-2-(ethoxycarbonyl)-, perchlorate収率 76%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To 30 ml of tetrahydrofuran, 1.4 g of proline ethyl ester was dissolved, and 2.0 g of 2-methylthio-1,3-dithiolium perchlorate was gradually added under stirring at room temperature. The mixture was stirred at room temperature for 1 hour, and the precipitated crystals were collected by filtration and recrystallized from methanol-ethyl ether, whereby 2.1 g (yield: 76%) of 1-(1,3-dithiol-2-ylidene)-2-ethoxycarbonylpyrrolidinium perchlorate (Compound No. 41) was obtained as crystals having a melting point of from 113° to 114° C.

後処理

  1. stirringThe mixture was stirred at room temperature for 1 hour
  2. filtrationthe precipitated crystals were collected by filtration
  3. customrecrystallized from methanol-ethyl ether

出典と根拠

ORDレコード
ord-cd9d47d9f12b488ebb9f4d7c3af38431
出典データセット
uspto-grants-1988_04
特許番号
US04737494

関連ノート

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